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High Throughput Experimentation Using DESI-MS to Guide Continuous-Flow Synthesis.

Bradley P Loren1, H Samuel Ewan1, Larisa Avramova1

  • 1Department of Chemistry, Purdue University, Purdue University Center for Cancer Research, Multi-disciplinary Cancer Research Facility, Bindley Bioscience Center, 1203 W. State Street, West Lafayette, IN, 47907, USA.

Scientific Reports
|October 16, 2019
PubMed
Summary
This summary is machine-generated.

Desorption electrospray ionization mass spectrometry (DESI-MS) accelerates reaction optimization by predicting microfluidic reaction outcomes. This high-throughput method efficiently narrows down chemical reaction parameters for faster synthesis development.

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Area of Science:

  • Analytical Chemistry
  • Organic Synthesis
  • Chemical Engineering

Background:

  • Accelerating reaction optimization is crucial for developing efficient continuous-flow syntheses.
  • High-throughput experimentation (HTE) methods are needed to rapidly explore chemical reactivity.
  • Validating predictive models across different reaction platforms is essential for reliable optimization.

Purpose of the Study:

  • To demonstrate the utility of desorption electrospray ionization mass spectrometry (DESI-MS) for predicting microfluidic reaction outcomes.
  • To establish a predictive connection between DESI-MS, batch, and microfluidic reaction conditions.
  • To explore how DESI-MS HTE can identify trends in reactivity across various parameters.

Main Methods:

  • Utilized DESI-MS as an HTE tool for qualitative prediction of reaction outcomes.
  • Investigated N-alkylation reactions as a model system due to ESI-MS detectability.
  • Compared reaction trends across DESI-MS, batch, and microfluidic platforms, analyzing parameters like solvent, temperature, and stoichiometry.

Main Results:

  • DESI-MS HTE effectively predicted microfluidic reaction outcomes, narrowing the search space for optimization.
  • Identified trends in reactivity based on chemical structure, solvent, temperature, and stoichiometry.
  • While DESI-MS guided solvent selection, parameters like stoichiometry and temperature still required optimization in continuous synthesis.

Conclusions:

  • DESI-MS HTE significantly reduces the time and materials needed for optimizing chemical reactions.
  • This approach accelerates the development of efficient continuous-flow syntheses.
  • DESI-MS serves as a valuable tool for rapid exploration and optimization of chemical reactivity.